The glycoprotein, skeletal muscle (-dystroglycan, was analyzed for monosaccharide composition by preparing the TMS derivatives of the methylglycosides followed by GC and GC/MS analyses. TMS methylglycosides were prepared from the sample by methanolysis in 1 M HCl in methanol, followed by N-acetylation with pyridine and acetic anhydride. The sample was then treated with Tri-Sil. GC analysis of the TMS methylglycosides was done on an HP 5890 GC using a DB1 fused silica capillary column. GC/MS analysis was performed using a Hewlett Packard 5890 GC coupled to a 5970 MSD. Monosaccharides were identified by their retention times in comparison to standards, and their carbohydrate character was authenticated by their mass spectra.